Soap preparation



Aug. 7, 1945. J. Ross soAP PREPARATION Filed Aug. l5, 1942 i 9 l l 0 l 0a u l D n l I 0 O O O O O O O Q O O O O O ITmJ O C O O o O 0 O O 0 G O OG .v0 #000 Ilollllbl ITM. ,Q m. n. .N .H

Ilm.

. INVENTOR. 'L/OHA/ @0.55.

ATTORNEY Patented ug. 7, 1945 SOAP PREPARATION John Boss, Ramsey, N..J., assignor toColgate- Palmolive-Peet Company, Jersey City, N. J., a

corporation of Delaware Application August 15, 1942, Serial No. 454,909

Claims.

The present invention relates to a method for converting moltenanhydrous soap to a readily usable form and, more particularly, to aprocess for cooling and partially hydrating molten. anhydrous soap, toan apparatus therefor, and to the product of said process.

- Anhydrous soap has been made by various ing the molten soap into andbeneath the surface of a pool of water or soap 4solution and intimatelymixing the soap therewith, but this method provides a soap containing a,large amount of water, part of which mustfrequently be'removed, as whenit is desired to make a milled soap. The removal of the water is acostly and time-consuming operation and requires equipmentwhich occupiesconsiderable space, all of which-are disadvantageous. It has also beensuggested to cool the soap out of contact with air by carrying itthrough a pipe by means of a worm conveyor, the solid anhydrous soapcoming out as chips at the outlet end of the pipe. This method has thedisadvantage that the solid anhydrous soap is extremely'diillcult towork and/or to dissolve, so that the soap is notin a. readily usableform.

, Thus, although these and other suggestions and proposals have beenmade, no satisfactory method, so far as is known, has been provided forrapidly cooling molten anhydrous soap and converting it into a readilyusable form.

It is an object of the present invention to provide a novel method fordirectly and rapidly cooling molten anhydrous soap out of contact withair without substantial change of shape and with or without partiallyhydrating the soap.

l of eaclrstring is partially hydrated. The strings' A It is anotherobject of the invention to provide Other objects and advantages of thisinventionwill be apparent from the following description,

taken in conjunction with the accompanying drawing, wherein:

Fig. 1 shows a longitudinal sectional view, partly diagrammatic, of anapparatus in accordance with the present invention; I I

Fig. 2 is-a fragmentary detail section taken' substantially on the line2-2 of Fig. 1; and

Fig. 3 depicts a transverse section taken onthe .line 3--3 of Fig. 2. L

According. to this invention, molten anhydrous soap is expressed in theform of threads or strings out of contact with air .into a pool ofcooling liquid. The molten soap is ecooled by contact with the liquid,and, when an aqueous body is employed as the cooling liquid, the outerportion are kept out of contact with each other for a short period Ioftime, during which cooling is' continued, and the illiform soap is thenremoved from the pool at a temperature where oxidation upon contact withair is substantially negligible and in a condition in which the soap canbe passed directly to mills and plodders for further processing. l Themolten anhydrous soap may be made by .any of the methods known to theart. Thus,

fats and fatty oils and/or free fatty acids and/or esters thereof may bemixed with alkaline agents in batch, intermittent or continuousoperation, and the resulting reaction mixture heated to somewhatelevated temperatures and then iiashed into a lower pressure zone tovolatilize Water or other solvents, glycerine (if any), alcohols (ifany), and unsaponiable matter and to recover the resulting anhydroussoap. In another method, the fatty material and alkaline agent areheated together in the absence of air and liquid water to a temperatureabove the melting point of the resulting anhydroussoap while passing acurrent of steam therethrough to remove glycerine, if any, andunsaponiiable matter. The alkaline or saponifying agents which may beused for saponifying these fatty materials include sodium and potassiumhydroxides, carbonates, silicates, etc., lime, magnesium carbonate,pyridine,v

methyl morpholine, alkyl amines, alkanolamines, and other organic andinorganic bases and al'- kaline materials, and mixtures of these; 'I'healkaline agent may be introduced in aqueous solution, in 'alcoholicsolution, or in solutions of other solvents, or may be substantiallyanhydrous and/or substantially undiluted. It will be understood from theforegoing that molten anhy drous soap made by any other. method would beequally applicable for treatment by the present in the soap so that itis sun fluid enough to be extruded through the orifices withoutcloggingthem.

The pool into which the molten anhydrous soap is expressed or extrudedmay be of water or other suitable liquid or may be an aqueous solutionof soap, sodium chloride, sodium sulphate, sodium carbonate and/or othermaterial capable of decreasing the solubility of the soap in the water.A non-solvent for soap, such as an alkanel cycloalkane, ether orhalogenated alkane or ether, may similarly be employed as the coolingliquid. The orifices may be of any desired size and shape and may beuniform or not, as desired. In general,

round orifices of about JAG inch to about 1/2 inch or larger arepreferred, and 1/4 inch orifices have been found to give satisfactoryresults. The orifices are preferably spaced apart by a distance of abouttwice to about ten times their own diameters to keep the strings of soapout of contact with each other for a short time.

Another method of keeping the strings apart is to surround eachoricewitha short tube larger in diameter than the orifice and open atone end to the solution in the cooling vessel.

in individual strings for as long a time as is desired before allowingthem to come into contact with each other, and such length willnecessarily depend upon such factors as the temperatures of the soap andof the cooling liquidand the speed at which the soap is extruded, aswill be apparent to those skilled in the art.

Since the Adifference in temperature between the molten anhydrous soapand the cooling liquid is necessarily great, the temperature differencenormally being over 200 C., itis preferred to provide means for keepingthe cooling liquid in motion. Such means may comprise stirrers andagitators in the`cooling liquid, or, where practicable, it is preferredto flow the cooling uid across the path of travel of the soap strings.Where tubes surrounding the orifices are employed, the tubes may beperforated to permit fresh cooling liquid to come into contact with thehot soap. This has the further advantage of sweeping away the vaporwhich is usually formed upon contact of the soap with the cooling fluid.

The processof the invention will now be described in connection withl anovel apparatus for carrying the same into practice. Referring to thefigures, reference character I designates a molten anhydrous soap supplyvessel, the outlet of which is connected by means of a conduit with theinlet The length of these tubes may be adjusted to keep the soap` 9A ofdiameter larger than the orices 8 in the wall are perpendicularlyafiixed to the inner surface of said wall 6, the end of each tubesurrounding one of the orifices, and each tube has a plurality ofperforations l0. The other end of each tube is open in the coolingvessel 1. A continuous mesh conveyor Il is provided in the vessel, saidconveyor being at least as wide as the bank of tubes and being mountedin a position vabove said tubes and adapted to move material along thebottom of said conveyor in the same longitudinal direction as from theclosed to the open ends of said tubes. A belt conveyor l2 ofapproximately the same width as the conveyor Il and extending insubstantially the same direction is mounted with its lower end beneaththe forward end of the conveyor Il' and with its upper end outside thecooling vessel and said conveyor 'l 2 is adapted to carry material uponthe upper surface thereof. Means (not shown in the figures) areprovidedfor driving the conveyors. A liquid inlet l 3 is provided at the bottomi4 of the Vessel 'l near a side thereof perpendicular to wall 6, and apump is adapted to y deliver cooling liquid to this inlet at a desiredrate. An yoverflow outlet at the opposite side of the cooling vessel isprovided for removal of the heated liquid. The overflow may be cooled,adjusted to proper composition with make-up water, solution, etc., andrecirculated through the pump, if desired.

The operation of the dvice is relatively simple and will now bedescribed in connection with the use of an aqueous body as thecoolingliquid therein. Molten anhydrous soap is removed from the supply vessell by the pump 2 and delivered to the heat exchange unit 4, where part ofthe heat in the soap is removed. Sufficient heat remains so that thesoap'in molten, semi-molten, plastic or semi-plastic form can be forcedunder pressure into the manifold 5 and through the orifices 8 in thewall 6 of the cooling vessel 1. The soap is expressed through theorifices 8 into the tubes 9. At the start of the operation, since thetubes are open at one end thereof to the aqueous cooling liquid in thevessel, the tubes are filled with the cooling liquid. When the hotanhydrous soap comes into contact with the aqueous liquid in the tubes,steam is formed, and an envelope of steam attaches itself to the stringsof soap. The steam tends to make the soap rise in the cooling liquid,especially where a heavy` brine of a pump 2 driven .by a motor 3. Theoutlet of the pump connects by means of a conduit with .a

heat exchange unit 4, and a pipe from this unit leads to a` manifold orheader 5 attached to thelower portion of the outside of a wall 6 of acooling vessel 1. The wall 6 is perforated at its lower portion with aplurality ofA orifices 8, all of which are within the area covered bythe mainfold 5 upon the outside Vof the Wall. A pluraiity of tubes`tions at the lower sides.

solution is employed, and the strings of soap of anhydrous soap withinthel string; Where the factors which influence the rate ofy cooling, aswill be discussed infra, are such that the strings of soap aresufficiently cooled so that they will not conglomerate upon comingtogether, the strings -emerge from the open end of the tubes 9 and areindividually carried up by the steam envelope around them to theunder-surface of the'conveyor Il. They are carried along bythe conveyoruntil the steam which surrounds them has escaped through the mesh of theconveyor into the 4 upper portion of the cooling vessel, and the fstrings then fall uponthe upper side of the conbefore flashing orheating or by simultaneously veyor I2. This second conveyor removes themfrom'the vessel.

The number, size and spacing of the orifices in. y

the wall of the'cooling vessel, the length ofthe tubes provided, thespeed at which the strings of soap move through the liquid. as well asthe rate at which the cooling liquid is circulated through the vessel,the temperature of the cooling liquid, the amount of prec'ooling of thehot anhydrous soap before extrusion through the 'oriiices, the totallength of time that the soap stays in the cooling vessel, etc., areamong the liform soap may be fed directlyto mills and plodders, there tohave adjuvant materials incorporated therewith. Where the variousfactors are so adjusted that soap will conglomerate upon coming togetherto form a partially hydrated mass of soap, the amount of hydration canalso be controlled to provide a soap which can be directly milled andplodded.

When it isdesired to produce a substantially anhydrous product, anon-aqueous cooling liquid, preferably a high-boiling organic liquid inwhich the soap is substantially insoluble, may be employed, asaforesaid. The soap, after cooling, may be blown to volatilize the filmof liquid thereon, especially if the liquid employed is relativelylow-boiling, or such film may be removed by extraction with alow-boiling solvent for the liquid, which solvent may be removed from'the soap in turn by blowing, slight heating or like methods. Thus,white oil, kerosene, decalin and/or tetralin may be used as the coolingliquid, and the residual film upon the iliform soap may be extractedwith ethyl ether, petroleum ether and/or other volatile solvent.

Adjuvant materials which may be mixed with' the soap include fatty acidsoaps prepared by the same or other methods, resin acid soaps,naphthenic and alkylated naphthenic acid soaps, sulphated andsuiplionated organic compounds, alkaline soap builders, water-soluble,water-softening acid compounds of phosphorus, and other salts includingsodium carbonate, sodium siliflashing a second solution containing suchadjuvant materials.

The present process has the advantage vof cooling anhydrous soap out ofcontact with air so that decomposition and discoloration of the productare avoided, while simultaneously hydrating the soap to a desiredamountsuitable for processing without having to remove part ofthe Water. Afurther advantage of the process ist'o provide soap in a convenientand'easily handled form which may be ,easily dissolved or which may beused directly' in mills and plodders `in the manufacture of a milledsoap.

It will be understood that the term molten as applied herein to theanhydrous soap treated is also intended to include said vsoap in s'emi-vmolten, plastic, and semi-plastic forms.

Although the present invention has been described in connection With a.particular embodiment, it will be understood by those skilled'v in theart that other variations and modifications of the invention can be madeand that various equivalents can be substituted therefor withoutdeparting from the yprinciples disclosed herein. Thus, instead ofintroducing the molten soap at the side of the pool of cooling l-iquid,`the orinces may be positioned at either the top or the bottqm of thepool, depending upon the gravity and boilingpoint of the liquidrused andwhether the strtngs of soap will at first tend to fall or to rise uponbeing extruded into the cooling liquid.

cates, trisodium phosphate, borax, sodium tetraphosphate, sodiumbicarbonate, sodium sulphate, sodium chloride, sodium acetate, sodiumhypochlorite, sodium thiosulphate, sodium perborate,

, sodium tartrate, sodium citrate and sodium oxalate, and thecorresponding-ammonium, substituted ammonium and potassium salts of thecorresponding acids; insecticidal, germicidal, styptic and medicinalagents, including aluminum chloride, mercurio chloride and variouscopper and K lead salts; coloring agents, abrasives, llers, and

water-dispersible gums, including dyes, lakes,

pigments, silica,` kieselguhr, silica gel, feldspar,

precipitated chalk, pumice, infusorial earth, bentonite, talc, starch,Irish moss, sugar, methyl cellulose, agar, gum tragacanth, gum arabic,and polyvinyl alcohol; liquids, such as ethyl alcohol, glycerol,cyclohexanol, naphtha, benzene, kerosene, turpentinefpine oil, decalinand tetralin and `I the like. The type of addition-agent will dependupon the ultimate use of the new composition. Other ways ofincorporating these addition agents besides mixing the final' producttherewith are to admix the adjuvant materials with the raw fattymaterial and/or the saponifying agents Such arrangement may sufiice insome cases to keep the strings separated from each otherfuntil cool. Itwill also be appreciated that, although the extruded soap has beendescribed as in filamentous form, the orifices may be of .such shape anddimensions that ribbons, sheets, and the like can be produced. 'Iheseand other variations and modicationsare believed to be within the scopeof the present specification and within the purview of the appendedclaims.

I claim:

1. A process of treating molten anhydrous soap which comprises extrudingmolten anhydrous soap through a plurality of orifices into a body o f anaqueous cooling liquid, maintaining the strings of soap so formed out ofcontact with each other for ,a time intervalv sulcient for cooling saidstrings below the temperatures of substantial conglomeration and ofsubstantial oxidation in the presence of air and insuiiicient forsubstantially changingv the shape of the. soap and for more thanpartially hydrating said soap, and resoap out of contact with anoxidizing medium through a plurality of oriicesinto and below thesurface of a body of an aqueous cooling liquid, maintaining said soapextrusions therein out of contact with eachother until partiallyhydrated and cooled below the temperature of substantial conglomeration,andremovingv said partially hydrated soap fromsaid liquid ,body withoutsubstantial change in shape.

3. A process of treating molten anhydrous soap which comprises passingcontinuous strings of molten anhydrous soap through a body of an aqueouscooling liquid, maintaining said strings therein out of contact witheachother until partially hydrated and cooled below the temperature vofvsubstantial conglomeration, continuously removing said partiallyhydrated soap in filamen- 4 f a i 2,381,368

tous form from said liquid body, and milling and plodding said filiformsoap.

4. A process of treating molten anhydrous soap which comprises extrudingmolten anhydrous soap out of contact with an oxidizing'medium through aplurality of orices into and below the surface of a body of ahigh-boiling organic liquid wherein the soap is substantially insoluble,maintaining saidsoap extrusions therein out of contact with each otheruntil cooled below the temperature of substantial conglomeration,removing said soap from said organic liquid body without substantialchange in shape, washing said soap with a volatile-organic solventwherein residual high-boiling organic liquid upon said soap is solubleand wherein the soap is substantially insoluble, and vaporizing residualvolatile solvent from said soap. A

5. A process of treating moltenanhydrous soap which comprises extrudingthe molten anhydrous soap through a .plurality of orifices into a bodyof a cooling liquid, maintaining the strings of soap so formed out ofcontact with each other for a time sulcient for cooling said stringsbelow the temperature of substantial conglomeration, andJ removing saidcooled soap from said body of liquid.

JOHN ROSS.

